CN105541340B - Nitride ceramics-glass ceramic composite and preparation method thereof - Google Patents
Nitride ceramics-glass ceramic composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of nitride ceramics glass ceramic composite and preparation method thereof, which fires after being mixed by the silica of the silicon nitride of 20~90wt.%, the boron oxide of 10~70wt.% and 0~70wt.% and forms；Wherein boron oxide is obtained by boric acid dehydration conversion.Its preparation method using wet method mix grinding to uniform, obtains slurry first to weigh raw material；Then dry, load mould after obtaining solid powder, 1~3h is kept the temperature in 200~700 DEG C under the conditions of vacuum or inert gas shielding, then heated up with the speed of 5~20 DEG C/min；When temperature rises to 1550~1850 DEG C, pressurization, maintains pressure in 5~20MPa hot pressing, 1~3h；Cooling, the demoulding, obtain the nitride ceramics glass ceramic composite.This method short preparation period, yield is high, and it is homogeneous that properties of product are made.
Description
Technical field
The present invention relates to inorganic composite materials field, more particularly to a kind of nitride ceramics-glass ceramic composite
And preparation method thereof.
Background technology
Nitride ceramics-glass ceramic composite is sent out on the basis of silica glass material and boron nitride ceramic material
The new material that exhibition is got up.This material combines the advantages of quartz glass and boron nitride, has the two in microstructure again
Structure is closed, while the two dielectric properties is kept, also with excellent thermal protective performance, wave transparent performance, ablation resistance and power
Performance is learned, anti-warmware and communication window available for manufacture superelevation velocity of sound aircraft.However, although some existing techniques can
Synthesize such composite material of excellent performance, but technique is cumbersome, and cost is higher.Harbin Institute of Technology Zhang Junbao is won for 2001
Scholar's thesis《The sol-gel of Si-B-O-N powder prepares and its structure property of ceramics》It is middle to select trichlorine boron azine and gather
Chlorine oxosilane is the precursor of boron nitride and silicon oxynitride, and both are prepared by crosslinking agent of ammonia again by MOLECULE DESIGN than mixing
The gel stablized, then gel cracks to obtain the non-crystalline flour of nitride ceramics, finally carry out hot pressing at different temperatures, prepares
Hardness, bending strength and fracture toughness are respectively 26.7GPa, 202MPa and 3.43High-performance boron nitride/micro-
Crystal glass composite ceramic material.《Alloy and compound periodical》The paper of the 244-253 pages publication of volume 232 in 1996《Pass through
Tropical resources polyborosiloxane prepares the characterization of boron silicon oxynitride》, i.e. L.Bois, P.L'Haridon,
Y.Laurent.Characterization of a boro-silicon oxynitride prepared by thermal
nitridation of a polyborosiloxane.Journal of Alloys and Compounds,1996,232:
244-253；It is middle that boron silicon-oxygen polymer is generated using boric acid and silicon tetrachloride reaction, nitrogenized in ammonia air-flow and obtain such material
Material.These techniques all exist prepare used in the cycle it is longer, poor repeatability, yield is relatively low, the craftsmanship such as what quality was not easily controlled
Problem, so as to limit the practical application of the material.
The content of the invention
In order to solve the above technical problem, the present invention provides a kind of nitride ceramics-glass ceramic composite and its system
Preparation Method, this method short preparation period, yield is high, and it is homogeneous that properties of product are made.
For this reason, technical scheme is as follows：
A kind of nitride ceramics-glass ceramic composite, fired after being mixed by following raw material according to mass percent and
Into：
Silicon nitride 20%~90%；
Boron oxide 10%~70%；
Silica 0%~70%；
Wherein boron oxide is obtained by boric acid dehydration conversion, and the quality of boron oxide converts according to the 56.3% of boric acid quality
Arrive.
The preparation method of the nitride ceramics-glass ceramic composite, includes the following steps：
1) raw material is weighed according to proportioning, using wet method mix grinding, using n-hexane or acetone as medium, raw material is mixed, is obtained
Slurry；
2) slurry is dried, obtains solid powder；
3) solid powder for obtaining step 2) loads mould, in 200~700 under the conditions of vacuum or inert gas shielding
DEG C 1~3h of insulation, is then heated up with the speed of 5~20 DEG C/min；
4) when temperature rises to 1550~1850 DEG C, pressurization, maintains pressure in 5~20MPa hot pressing, 1~3h；Cooling, take off
Mould, obtains the nitride ceramics-glass ceramic composite.
It is preferred that raw material is by the silicon nitride of 65~70wt.% and the boron oxide powder constituent of 30~35wt.%；In step 4)
Hot pressing condition is 1600 DEG C or 1700 DEG C or 1800 DEG C.
It is preferred that raw material is by the silicon nitride of 55~60wt.% and the boron oxide powder constituent of 40~45wt.%；In step 4)
Hot pressing condition is 1600 DEG C or 1700 DEG C or 1800 DEG C.
It is preferred that raw material is by the silicon nitride of 49~51wt.% and the boron oxide powder constituent of 49~51wt.%；In step 4)
Hot pressing condition is 1600 DEG C or 1700 DEG C or 1800 DEG C.
It is preferred that raw material is by the silicon nitride of 34~36wt.%, the boron oxide powder of 33~36wt.% and 27~31wt.%
SiO 2 powder forms；Hot pressing condition is 1700 DEG C in step 4).
It is preferred that raw material is by the silicon nitride of 42~45wt.%, the boron oxide powder of 28~32wt.% and 24~29wt.%
SiO 2 powder forms；Hot pressing condition is 1700 DEG C in step 4).
The present invention is formed using the solid phase reaction of boron oxide and silicon nitride at high temperature contains hexagonal boron nitride, titanium dioxide
Nitride ceramics-glass ceramic composite that silicon, silicon oxynitride and the things such as nitrogen oxidation boron are mutually formed, then by adding titanium dioxide
Silicon adjusts amorphous content and microstructure therein so as to improve the performance such as anti-thermal shock and resistance to ablation.Prepare in this way
Nitride ceramics-glass ceramic composite have technique it is simply efficient, component be easy to adjust control, material easily burn till and into
The advantages that being evenly distributed.
Brief description of the drawings
Fig. 1 is the material phase analysis result figure of product obtained by embodiment 2,10,14.
Embodiment
Technical scheme is described in detail with reference to embodiments.
Embodiment 1
A kind of preparation method of nitride ceramics-glass ceramic composite, includes the following steps：
1) raw material silicon nitride 68% and boron oxide powder 32% are weighed according to mass percent, wherein boron oxide is taken off by boric acid
Water converts to obtain, and the quality of boron oxide is obtained according to 56.3% conversion of boric acid quality；Load weighted silicon nitride and boric acid are put
Enter agate pot, according to ratio of grinding media to material 2:1 adds agate ball；Add grinding aid acetone or n-hexane；Mixed on planetary ball mill
Close 4 it is small when after obtain slurry；
2) slurry is dried into 2~4h under the conditions of 80~90 DEG C, removes ball-milling additive, grinding, cross 100 targets standard
Sieve, obtains solid powder；
3) solid powder for obtaining step 2) is fitted into the graphite jig that inner wall scribbles boron nitride, it is die-filling after the completion of by its
It is put into hot pressing furnace, keeps the temperature 1~3h in 450 DEG C under vacuum conditions, then under inert gas such as argon gas or nitrogen protection,
Heated up with the speed of 10 DEG C/min；
4) when temperature rises to 1600 DEG C, pressurization, maintains pressure in 10MPa hot pressing 2h；Cooling, the demoulding, take out agglomerate
Body, obtains the nitride ceramics-glass ceramic composite.
Embodiment 2
With the preparation method of nitride ceramics-glass ceramic composite in embodiment 1 difference lies in：
The raw material is by the silicon nitride of 57wt.% and the boron oxide powder constituent of 43wt.%；Boron oxide is turned by boric acid dehydration
Change obtains, and the quality of boron oxide is obtained according to 56.3% conversion of boric acid quality.
Other techniques are the same as embodiment 1.
Fig. 1 a obtain its thing phasor of product for the present embodiment；It can be seen that its structure is by fine grain boron nitride, devitrified glass composition.
Embodiment 3
With the preparation method of nitride ceramics-glass ceramic composite in embodiment 1 difference lies in：
The raw material is by the silicon nitride of 50wt.% and the boron oxide powder constituent of 50wt.%；Boron oxide is turned by boric acid dehydration
Change obtains, and the quality of boron oxide is obtained according to 56.3% conversion of boric acid quality.
Other techniques are the same as embodiment 1.
Embodiment 4
With the preparation method of nitride ceramics-glass ceramic composite in embodiment 1 difference lies in：Step 4) hot pressing
Temperature be 1700 DEG C, other techniques are the same as embodiment 1.
Embodiment 5
With the preparation method of nitride ceramics-glass ceramic composite in embodiment 2 difference lies in：Step 4) hot pressing
Temperature be 1700 DEG C, other techniques are the same as embodiment 2.
Embodiment 6
With the preparation method of nitride ceramics-glass ceramic composite in embodiment 3 difference lies in：Step 4) hot pressing
Temperature be 1700 DEG C, other techniques are the same as embodiment 3.
Embodiment 7
With the preparation method of nitride ceramics-glass ceramic composite in embodiment 1 difference lies in：Step 4) hot pressing
Temperature be 1800 DEG C, other techniques are the same as embodiment 1.
Embodiment 8
With the preparation method of nitride ceramics-glass ceramic composite in embodiment 2 difference lies in：Step 4) hot pressing
Temperature be 1800 DEG C, other techniques are the same as embodiment 2.
Embodiment 9
With the preparation method of nitride ceramics-glass ceramic composite in embodiment 3 difference lies in：Step 4) hot pressing
Temperature be 1800 DEG C, other techniques are the same as embodiment 3.
Embodiment 10
With the preparation method of nitride ceramics-glass ceramic composite in embodiment 1 difference lies in：
The raw material is made of the SiO 2 powder of the silicon nitride of 44wt.%, the boron oxide of 30wt.% and 26wt.%；
Boron oxide is obtained by boric acid dehydration conversion, and the quality of boron oxide is obtained according to 56.3% conversion of boric acid quality；Step 4) hot pressing
Temperature be 1700 DEG C.
Other techniques are the same as embodiment 1.
Fig. 1 b obtain its thing phasor of product for the present embodiment；It can be seen that its structure is by fine grain boron nitride, silicon nitride and micro-
Crystal glass forms.
Embodiment 11
With the preparation method of nitride ceramics-glass ceramic composite in embodiment 1 difference lies in：
The raw material is made of the SiO 2 powder of the silicon nitride of 44wt.%, the boron oxide of 43wt.% and 13wt.%；
Boron oxide is obtained by boric acid dehydration conversion, and the quality of boron oxide is obtained according to 56.3% conversion of boric acid quality；And step 4) heat
The temperature of pressure is 1700 DEG C.
Other techniques are the same as embodiment 1.
Embodiment 12
With the preparation method of nitride ceramics-glass ceramic composite in embodiment 1 difference lies in：
The raw material is made of the SiO 2 powder of the silicon nitride of 35wt.%, the boron oxide of 36wt.% and 29wt.%；
Boron oxide is obtained by boric acid dehydration conversion, and the quality of boron oxide is obtained according to 56.3% conversion of boric acid quality；And step 4) heat
The temperature of pressure is 1700 DEG C.
Other techniques are the same as embodiment 1.
Embodiment 13
With the preparation method of nitride ceramics-glass ceramic composite in embodiment 1 difference lies in：
The raw material is by the silicon nitride of 30wt.% and the boron oxide powder constituent of 70wt.%；Boron oxide is turned by boric acid dehydration
Change obtains, and the quality of boron oxide is obtained according to 56.3% conversion of boric acid quality；And the temperature of step 4) hot pressing is 1700 DEG C.
Other techniques are the same as embodiment 1.
Embodiment 14
With the preparation method of nitride ceramics-glass ceramic composite in embodiment 1 difference lies in：
The raw material is by the silicon nitride of 90wt.% and the boron oxide powder constituent of 10wt.%；Boron oxide is turned by boric acid dehydration
Change obtains, and the quality of boron oxide is obtained according to 56.3% conversion of boric acid quality；And the temperature of step 4) hot pressing is 1700 DEG C.
Other techniques are the same as embodiment 1.
Fig. 1 c obtain its thing phasor of product for the present embodiment；It can be seen that its structure is by silicon nitride, boron nitride, and crystallite glass
Glass forms.
Embodiment 15
With the preparation method of nitride ceramics-glass ceramic composite in embodiment 1 difference lies in：
The raw material is made of the SiO 2 powder of the silicon nitride of 20wt.%, the boron oxide of 10wt.% and 70wt.%；
Boron oxide is obtained by boric acid dehydration conversion, and the quality of boron oxide is obtained according to 56.3% conversion of boric acid quality；And step 4) heat
The temperature of pressure is 1700 DEG C.
Other techniques are the same as embodiment 1.
Contrast the prior art such as《The sol-gel of Si-B-O-N powder prepares and its structure property of ceramics》Described in
Trichlorine boron azine and polychlorostyrene oxosilane obtain collosol and gel for the precursor of boron nitride and silicon oxynitride by 48h.Using ammonia as point
Agent and thermal decomposition atmosphere, the Si-B-O-N powder cracked by 10h are solved, then block is prepared using the technique of hot pressed sintering
Body material.The preparation process that technology provided by the invention simplifies, shortens flow time, it is possible to provide one kind is efficiently easily prepared
Technique.
The performance comparison table of nitride ceramics-glass ceramic composite prepared by 1 different process of table
Claims (3)
1. a kind of preparation method of nitride ceramics-glass ceramic composite, it is characterised in that include the following steps：
1) raw material is weighed according to proportioning, using wet method mix grinding, using n-hexane or acetone as medium, raw material is mixed, obtains slurry；
Wherein described raw material is by the silicon nitride of 65~90wt.% and the boron oxide powder constituent of 10~35wt.%, wherein boron oxide
Obtained by boric acid dehydration conversion, the quality of boron oxide is obtained according to 56.3% conversion of boric acid quality；
2) slurry is dried, obtains solid powder；
3) solid powder for obtaining step 2) loads mould, in 200~700 DEG C of guarantors under the conditions of vacuum or inert gas shielding
1~3h of temperature, is then heated up with the speed of 5~20 DEG C/min；
4) when temperature rises to 1600 DEG C or 1700 DEG C or 1800 DEG C, pressurization, maintains pressure in 5~20MPa hot pressing, 1~3h；
Cooling, the demoulding, obtain the nitride ceramics-glass ceramic composite.
2. a kind of preparation method of nitride ceramics-glass ceramic composite, it is characterised in that include the following steps：
1) raw material is weighed according to proportioning, using wet method mix grinding, using n-hexane or acetone as medium, raw material is mixed, obtains slurry；
Wherein described raw material is by the silicon nitride of 55~60wt.% and the boron oxide powder constituent of 40~45wt.%, wherein boron oxide
Obtained by boric acid dehydration conversion, the quality of boron oxide is obtained according to 56.3% conversion of boric acid quality；
2) slurry is dried, obtains solid powder；
3) solid powder for obtaining step 2) loads mould, in 200~700 DEG C of guarantors under the conditions of vacuum or inert gas shielding
1~3h of temperature, is then heated up with the speed of 5~20 DEG C/min；
4) when temperature rises to 1600 DEG C or 1700 DEG C or 1800 DEG C, pressurization, maintains pressure in 5~20MPa hot pressing, 1~3h；
Cooling, the demoulding, obtain the nitride ceramics-glass ceramic composite.
3. a kind of preparation method of nitride ceramics-glass ceramic composite, it is characterised in that include the following steps：
1) raw material is weighed according to proportioning, using wet method mix grinding, using n-hexane or acetone as medium, raw material is mixed, obtains slurry；
Wherein described raw material is by the silicon nitride of 42~45wt.%, the boron oxide powder of 28~32wt.% and 24~29wt.%
SiO 2 powder forms, and wherein boron oxide is obtained by boric acid dehydration conversion, and the quality of boron oxide is according to boric acid quality
56.3% conversion obtains；
2) slurry is dried, obtains solid powder；
3) solid powder for obtaining step 2) loads mould, in 200~700 DEG C of guarantors under the conditions of vacuum or inert gas shielding
1~3h of temperature, is then heated up with the speed of 5~20 DEG C/min；
4) when temperature rises to 1700 DEG C, pressurization, maintains pressure in 5~20MPa hot pressing, 1~3h；Cooling, the demoulding, obtain described
Nitride ceramics-glass ceramic composite.
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Non-Patent Citations (2)
| Title |
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| Chemical Reactions in the System Si3N4-SiO2-B2O3;Anna-Karin etal.;《journal of the European Ceramic Society》;19971022;第633-640页 * |
| 温度对原位反应制备的Si–B–O–N 陶瓷微观结构及力学性能的影响;吴赟等;《硅酸盐学报》;20120930(第9期);第1265-1270页 * |
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